反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Methyl 3-(2-(dichlorophosphoryloxy)phenyl)propanoate, 81 (2.77 mmol) and L-alanine methyl ester hydrochloride (0.42 g, 2.77 mmol) were suspended in anhydrous dichloromethane (10 mL). Anhydrous triethylamine (0.37 mL, 2.77 mmol) and dichloromethane (5 mL) were added dropwise at −78° C. under nitrogen. Following the addition, the reaction mixture was slowly warmed to it and stirred overnight. The solvent was removed under reduced pressure; the solid was washed with anhydrous ether (20 mL×2), and filtered. The filtrate was concentrated to a residue to give crude product as an oil. Dilution with THF (2.77 mL) gave a 1 M solution, which was used in the following step without any further purification.
WORKUP
后处理
- additionthe addition
- temperaturethe reaction mixture was slowly warmed to it
- customThe solvent was removed under reduced pressure
- washthe solid was washed with anhydrous ether (20 mL×2)
- filtrationfiltered
- concentrationThe filtrate was concentrated to a residue
- customto give crude product as an oil